US4293326A - Glass coating - Google Patents

Glass coating Download PDF

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Publication number
US4293326A
US4293326A US06/049,155 US4915579A US4293326A US 4293326 A US4293326 A US 4293326A US 4915579 A US4915579 A US 4915579A US 4293326 A US4293326 A US 4293326A
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US
United States
Prior art keywords
face
process according
glass
coating
gaseous medium
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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US06/049,155
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English (en)
Inventor
Robert Terneu
Albert Van Cauter
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Flachglas Wernberg GmbH
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BFG Glassgroup GIE
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Publication of US4293326A publication Critical patent/US4293326A/en
Assigned to FLACHGLAS AKTIENGESELLSCHAFT reassignment FLACHGLAS AKTIENGESELLSCHAFT ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BFG GLASSGROUP
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/245—Oxides by deposition from the vapour phase
    • C03C17/2453—Coating containing SnO2
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/001—General methods for coating; Devices therefor
    • C03C17/002—General methods for coating; Devices therefor for flat glass, e.g. float glass

Definitions

  • This invention relates to a process of forming a tin oxide coating on a face of a glass substrate by contacting such face while it is at elevated temperature with a gaseous medium containing tin tetrachloride which undergoes chemical reaction and/or decomposition to form said tin oxide coating.
  • tin oxide coatings having very good optical properties and in particular a uniform light transmitting power, which implies a uniform structure of the coating.
  • the difficulty of achieving coatings of high optical quality are very appreciable if the coatings have to be formed continuously on a travelling substrate such as a glass ribbon and tend to be greater as higher substrate speeds are encountered.
  • a travelling substrate such as a glass ribbon
  • optical coatings on the flat glass during its continuous production and the tendency is for production speeds to increase.
  • float glass is produced at ribbon speeds of at least several meters per minute and speeds up to 12 meters per minute or more are attained in some plants.
  • the teaching derivable from the prior publications on chemical vapour deposition techniques does not enable tin oxide coatings of high optical quality to be reliably formed at high deposition rates on a glass substrate.
  • the formation of surface coatings by a chemical vapour deposition technique is influenced by numerous factors additional to the more obvious ones, namely the composition of the vapour and the nature of the vapour deposition reactions. Such other factors include the temperature conditions at the coating site, and the composition of the substrate face itself.
  • the rate of deposition of tin oxide on a travelling substrate made of glass can be increased by performing the coating operation in a moist atmosphere, the moisture level has to be very restricted when following the teaching of the prior publications, otherwise the results are unsatisfactory.
  • the coatings exhibit objectionable internal haze and indeed this was to be expected from the aforesaid United Kingdom specification 702,774 because the occurrance of haze is referred to in that specification as a reason why the amount of water vapour should be very restricted.
  • a process of forming a tin oxide coating on a face of a glass substrate or of a previously formed coating thereon by contacting such face while it is at elevated temperature with a gaseous medium containing tin tetrachloride which undergoes chemical reaction and/or decomposition to form said tin oxide coating, characterised in that said gaseous medium contains tin tetrachloride in a concentration corresponding to a partial pressure of at least 2.5 ⁇ 10 -3 atm. and contains water vapour in a concentration corresponding to a partial pressure of at least 10 ⁇ 10 -3 atm. and contains water vapour in a concentration corresponding to a partial pressure of at least 10 ⁇ 10 -3 atm. and is caused to contact said face while the temperature of the gaseous medium is at least 300° C. and the temperature of the glass where such contact occurs is above 550° C.
  • the FIGURE shows a cross-sectional side elevation of a coating station along the path of a ribbon of glass formed by the float process.
  • the gaseous medium is caused to flow along the substrate face being coated. This feature is responsible for a still further improvement in the coating quality which can be obtained.
  • the gaseous medium is caused to flow along the substrate face to be coated, as a substantially turbulence-free layer along a flow passage which is defined in part by the face of the glass and which leads to an exhaust ducting via which residual medium is drawn away from said face.
  • the avoidance of spurious deposits on the face to be coated are more easily avoided if the flow passage within which the coating is formed is shallow.
  • the height of the flow passage measured normally to the substrate face is at no point in excess of 40 mm.
  • the flow passage may be of uniform height or the passage may increase or decrease in height along its length in the direction in which the gas flow takes place.
  • the height of the flow passage is advantageous for the height of the flow passage to decrease in the direction of gas flow therethrough, at least over an end portion of its length leading up to the exhaust ducting.
  • the flow passage tapers over at least the greater part of its length.
  • An angle of taper of 10° or less is usually satisfactory.
  • the partial pressure of tin tetrachloride in the gaseous medium in contact with the face to be coated is from 2.5 ⁇ 10 -3 to 10 -2 atm.
  • high tin oxide deposition rates of at least 800 A/sec, even rates of between 2000 and 3000 A/sec., can be achieved with high process efficiency.
  • the minimum concentration of tin tetrachloride, within that range, which is required to achieve those results, and therefore the process efficiency, is dependent on the water vapour concentration.
  • Very high deposition rates of at least 800 A/sec, even e.g. between 2000 and 3000 A/sec as above referred to can be achieved while working within the above specified tetrachloride concentration range, by maintaining a water vapour concentration corresponding with a partial pressure of between 50 ⁇ 10 -3 and 200 ⁇ 10 -3 atm.
  • tin tetrachloride and water vapour are supplied to the coating zone in separate gas streams so that they come into contact in the vicinity of the substrate face being coated.
  • the tin tetrachloride vapour is preferably delivered to the substrate in a stream of nitrogen as carrier gas.
  • a stream of nitrogen containing tin tetrachloride vapour is caused to flow along the face being coated and a stream of air containing water vapour is delivered into that stream at a position where it is in flow along the said face.
  • a doping agent e.g. hydrogen fluoride
  • Such doping agent can, e.g., be fed to the substrate face being coated, mixed with moist air, or be fed separately.
  • the temperature of the glass at the coating zone can be appreciably above the specified lower limit of 550° but in accordance with common practice in the coating of glass by chemical vapour deposition techniques the temperature of the glass at the place where deposition occurs should not be so high that the glass is in soft condition.
  • the potential benefits of the invention are best realised when it is used for forming coatings at high deposition rates.
  • Very important processes according to the invention are those wherein the concentrations of tin tetrachloride and water vapour in the coating zone are such that a tin oxide coating is formed at a rate of at least 800 A/sec. Due to the high deposition rates which are attainable the invention can be employed with great advantage for forming a tin oxide coating on a ribbon of float glass as it travels from the float tank.
  • a ribbon of float glass is coated with tin oxide by contacting the ribbon with a gaseous medium as hereinbefore specified, at a region along the glass ribbon path where the temperature of the glass is in the range 550° to 650° C., the glass ribbon having a speed of at least 6 m/min, and the instantaneous amounts and concentrations of tin tetrachloride and water vapour in the gaseous medium from which the tin oxide deposition takes place being such that the coating forms on the substrate at a rate of at least 800 A/sec.
  • the coating formed by the process of the invention can be formed directly on the glass or on a previously formed coating.
  • a tin oxide coating can be formed by a process according to the invention on a relatively thin undercoating of another material, which may be helpful in avoiding haze due to structural phenomena at an interface.
  • a process according to the invention can of course be performed repetitively to form one tin oxide coating on another.
  • the illustrated coating apparatus was used for coating a ribbon of glass 1 travelling in the direction indicated by arrow 2 from a float tank (not shown) in which the glass ribbon was formed by a float process, on a bath of molten tin.
  • the glass ribbon had a speed of 12 meters per minute and was supported at the coating station by rollers 3.
  • the coating station is located in a compartment 4 of a horizontal gallery having a refractory roof 5 a refractory sole wall 6 and refractory side walls only one of which, designated 7, appears in the drawing.
  • the ends of the compartment are formed by displaceable refractory screens 8,9.
  • the coating apparatus is disposed at a position between the float tank and an annealing gallery. In an alternative mode, the coating apparatus could be disposed within a part of the annealing gallery.
  • the coating apparatus comprises three feed conduits 10,11,12 via which streams of gas can be delivered into the coating compartment.
  • the lower end portions of these conduits are inclined downwardly and forwardly in the direction of travel of the glass ribbon, at an angle of 45° to the horizontal.
  • the discharge ends of the conduits open into a shallow flow passage 13 defined in part by a shroud 14 and in part by the top face of the glass ribbon.
  • the shroud 14 extends across substantially the full width of the glass ribbon and the conduits 10,11,12 are of elongate rectangular cross section in the horizontal plane, their width (measured normally to the plane of the drawing) being only slightly less than the corresponding dimension of the shroud.
  • the inclined discharge end portions of such conduits define slot-like discharge passageways from which the gas streams issue in the form of layers extending over substantially the full internal width of the flow passage 13.
  • the top of the shroud 14 is inclined slightly downwardly in the gas flow direction so that the gas flow passage 13 slightly decreases in height towards its gas exit end at which it is connected to a chimney 15.
  • the length of the reactor, from the gas discharge end of conduit 12 to the chimney 15 is about 2 meters and its height varies from 40 mm at its entry end to 10 mm at its gas exit end.
  • the chimney 15 is internally subdivided by partitions such as 16 into a plurality of exhaust passageways distributed in side by side relationship across substantially the whole width of the gas exhaust path.
  • the temperature of the glass ribbon at the region beneath the entry end of the flow passage 13 was about 580° C.
  • Nitrogen pre-heated to 500° C. was fed from a source (not shown) along the duct 10 so as to serve as a kind of pneumatic screen isolating the passageway 13 from the gases located in the compartment 4 and externally of the shroud 14.
  • Tin tetrachloride vapour entrained in a stream of nitrogen at 450° C. was fed continuously along duct 11 so as to discharge as a stream flowing along the passageway 13.
  • the tin tetrachloride vapour was formed by spraying liquid tetrachloride into a pre-heated stream of nitrogen.
  • the duct 12 was continuously supplied with a gas mixture at 450° C. and comprising air, water vapour and hydrofluoric acid.
  • the purpose of the hydrofluoric acid was to dope with fluoride ions the coating forming on the glass ribbon so as to increase the far infrared reflectivity of the coating.
  • the supply of gas through duct 12 assists to move or press the reactive stream containing tin tetrachloride towards the surface of the glass.
  • the invention is carried out by causing the reactive gaseous medium to flow along the substrate face being coated.
  • This procedure although preferred is not essential.
  • tin tetrachloride vapour and water vapour and hydrofluoric acid can be blown in separate streams towards the glass ribbon and so as to mix in a zone in which they make contact with the glass and from which surplus gases, including reaction products, are withdrawn in a direction away from the glass ribbon.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)
  • Chemical Vapour Deposition (AREA)
US06/049,155 1978-07-20 1979-06-18 Glass coating Expired - Lifetime US4293326A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB30589/78 1978-07-20
GB7830589 1978-07-20

Publications (1)

Publication Number Publication Date
US4293326A true US4293326A (en) 1981-10-06

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Family Applications (1)

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US06/049,155 Expired - Lifetime US4293326A (en) 1978-07-20 1979-06-18 Glass coating

Country Status (11)

Country Link
US (1) US4293326A (es)
JP (1) JPS5515995A (es)
BE (1) BE877465A (es)
CA (1) CA1138725A (es)
DE (1) DE2929092A1 (es)
DK (1) DK154823C (es)
ES (1) ES482995A1 (es)
FR (1) FR2456077A1 (es)
IT (1) IT1120990B (es)
NL (1) NL189909C (es)
SE (1) SE440074B (es)

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4371740A (en) * 1980-07-23 1983-02-01 Eastman Kodak Company Conductive elements for photovoltaic cells
DE3638426A1 (de) * 1985-12-20 1987-07-02 Glaverbel Verfahren und vorrichtung zur ausbildung eines metalloxidueberzuges auf einem heissen glassubstrat
US4728353A (en) * 1985-12-20 1988-03-01 Glaverbel Process and apparatus for pyrolytically coating glass
US4880698A (en) * 1985-12-20 1989-11-14 Glaverbel Coated flat glass
US5022905A (en) * 1988-10-14 1991-06-11 Pilkington Plc Method and apparatus for coating glass
US5102691A (en) * 1989-09-20 1992-04-07 Atochem North America, Inc. Method of pretreatment for the high-deposition-rate production of fluorine-doped tin-oxide coatings having reduced bulk resistivities and emissivities
US5393563A (en) * 1991-10-29 1995-02-28 Ellis, Jr.; Frank B. Formation of tin oxide films on glass substrates
US5683516A (en) * 1994-07-18 1997-11-04 Watkins-Johnson Co. Single body injector and method for delivering gases to a surface
ES2111418A1 (es) * 1993-01-11 1998-03-01 Glaverbel Dispositivo y procedimiento para formar un recubrimiento porpirolisis.
WO1999004059A1 (en) * 1997-07-14 1999-01-28 Silicon Valley Group Thermal Systems, Llc Single body injector and deposition chamber
US6200389B1 (en) 1994-07-18 2001-03-13 Silicon Valley Group Thermal Systems Llc Single body injector and deposition chamber
US6354109B1 (en) * 1995-07-12 2002-03-12 Saint-Gobain Glass France Process and apparatus for providing a film with a gradient
US20070054044A1 (en) * 2003-07-10 2007-03-08 Sumitomo Titanium Method for forming metal oxide coating film and vapor deposition apparatus
US20090104369A1 (en) * 2006-03-27 2009-04-23 Beneq Oy Method for producing functional glass surfaces by changing the composition of the original surface
US20090165715A1 (en) * 2007-12-27 2009-07-02 Oh Jae-Eung Vapor deposition reactor
US20100041213A1 (en) * 2008-08-13 2010-02-18 Synos Technology, Inc. Vapor Deposition Reactor For Forming Thin Film
US20110076421A1 (en) * 2009-09-30 2011-03-31 Synos Technology, Inc. Vapor deposition reactor for forming thin film on curved surface
US8758512B2 (en) 2009-06-08 2014-06-24 Veeco Ald Inc. Vapor deposition reactor and method for forming thin film
US8840958B2 (en) 2011-02-14 2014-09-23 Veeco Ald Inc. Combined injection module for sequentially injecting source precursor and reactant precursor

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4670139B2 (ja) * 2000-11-22 2011-04-13 旭硝子株式会社 コーティング装置および方法
KR101244674B1 (ko) * 2006-05-02 2013-03-25 다우 코닝 아일랜드 리미티드 웹 밀봉 장치

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2651585A (en) * 1949-06-25 1953-09-08 Pittsburgh Plate Glass Co Production of electroconductive articles
GB702774A (en) 1951-05-08 1954-01-20 Pittsburgh Plate Glass Co Electro-conductive products and production thereof
US2953483A (en) * 1956-08-13 1960-09-20 Owens Illinois Glass Co Method and apparatus for applying coatings to selected areas of articles
US3632429A (en) * 1970-06-30 1972-01-04 Matsushita Electric Ind Co Ltd Method for making metal oxide film resistors
US4123244A (en) * 1976-04-13 1978-10-31 Bfg Glassgroup Process of forming a metal or metal compound coating on a face of a glass substrate and apparatus suitable for use in forming such coating

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE971957C (de) * 1953-06-07 1959-04-23 Pittsburgh Plate Glass Co Verfahren zur Herstellung elektrisch leitender Schichten auf Glas oder anderen waermebestaendigen Stoffen
BE632267A (es) * 1962-05-17 1900-01-01
DE1496590C3 (de) * 1964-10-16 1973-10-31 N.V. Philips' Gloeilampenfabrieken, Eindhoven (Niederlande) Verfahren zur Herstellung von warme reflektierenden SnO tief 2 Schichten mit reproduzierbaren optischen und elektrischen Eigenschaften auf Tragern
US3516811A (en) * 1966-10-04 1970-06-23 Indian Head Inc Method of and apparatus for coating glassware retaining its heat of formation
SU621647A1 (ru) * 1976-12-30 1978-08-30 Гусевский Филиал Государственного Научно-Исследовательского Института Стекла Способ обработки стеклоизделий

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2651585A (en) * 1949-06-25 1953-09-08 Pittsburgh Plate Glass Co Production of electroconductive articles
GB702774A (en) 1951-05-08 1954-01-20 Pittsburgh Plate Glass Co Electro-conductive products and production thereof
US2953483A (en) * 1956-08-13 1960-09-20 Owens Illinois Glass Co Method and apparatus for applying coatings to selected areas of articles
US3632429A (en) * 1970-06-30 1972-01-04 Matsushita Electric Ind Co Ltd Method for making metal oxide film resistors
US4123244A (en) * 1976-04-13 1978-10-31 Bfg Glassgroup Process of forming a metal or metal compound coating on a face of a glass substrate and apparatus suitable for use in forming such coating

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Ghoshtagore, "Mechanism of CVD Thin Film SnO.sub.2 Formation", J. Electrochem. Soc. Solid State Science and Technology, vol. 125, No. 1, Jan. 1978, pp. 110-117. *
Ghoshtagore, "Mechanism of CVD Thin Film SnO2 Formation", J. Electrochem. Soc. Solid State Science and Technology, vol. 125, No. 1, Jan. 1978, pp. 110-117.

Cited By (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4371740A (en) * 1980-07-23 1983-02-01 Eastman Kodak Company Conductive elements for photovoltaic cells
US4880698A (en) * 1985-12-20 1989-11-14 Glaverbel Coated flat glass
US4878934A (en) * 1985-12-20 1989-11-07 Glaverbel Process and apparatus for coating glass
DE3638426A1 (de) * 1985-12-20 1987-07-02 Glaverbel Verfahren und vorrichtung zur ausbildung eines metalloxidueberzuges auf einem heissen glassubstrat
DE3638426C2 (de) * 1985-12-20 1999-01-07 Glaverbel Verfahren und Vorrichtung zur Ausbildung eines Metalloxidüberzuges auf einem heißen Glassubstrat
US4728353A (en) * 1985-12-20 1988-03-01 Glaverbel Process and apparatus for pyrolytically coating glass
US5022905A (en) * 1988-10-14 1991-06-11 Pilkington Plc Method and apparatus for coating glass
US5102691A (en) * 1989-09-20 1992-04-07 Atochem North America, Inc. Method of pretreatment for the high-deposition-rate production of fluorine-doped tin-oxide coatings having reduced bulk resistivities and emissivities
US5393563A (en) * 1991-10-29 1995-02-28 Ellis, Jr.; Frank B. Formation of tin oxide films on glass substrates
US5487784A (en) * 1991-10-29 1996-01-30 Ellis, Jr.; Frank B. Formation of tin oxide films on glass substrates
ES2111418A1 (es) * 1993-01-11 1998-03-01 Glaverbel Dispositivo y procedimiento para formar un recubrimiento porpirolisis.
US5683516A (en) * 1994-07-18 1997-11-04 Watkins-Johnson Co. Single body injector and method for delivering gases to a surface
US6521048B2 (en) 1994-07-18 2003-02-18 Asml Us, Inc. Single body injector and deposition chamber
US5935647A (en) * 1994-07-18 1999-08-10 Wj Semiconductor Equipment Group, Inc. Method of manufacturing an injector for chemical vapor deposition processing
US6022414A (en) * 1994-07-18 2000-02-08 Semiconductor Equipment Group, Llc Single body injector and method for delivering gases to a surface
US6200389B1 (en) 1994-07-18 2001-03-13 Silicon Valley Group Thermal Systems Llc Single body injector and deposition chamber
US6354109B1 (en) * 1995-07-12 2002-03-12 Saint-Gobain Glass France Process and apparatus for providing a film with a gradient
WO1999004059A1 (en) * 1997-07-14 1999-01-28 Silicon Valley Group Thermal Systems, Llc Single body injector and deposition chamber
US20070054044A1 (en) * 2003-07-10 2007-03-08 Sumitomo Titanium Method for forming metal oxide coating film and vapor deposition apparatus
US20090104369A1 (en) * 2006-03-27 2009-04-23 Beneq Oy Method for producing functional glass surfaces by changing the composition of the original surface
US20090165715A1 (en) * 2007-12-27 2009-07-02 Oh Jae-Eung Vapor deposition reactor
US8333839B2 (en) * 2007-12-27 2012-12-18 Synos Technology, Inc. Vapor deposition reactor
US20100041213A1 (en) * 2008-08-13 2010-02-18 Synos Technology, Inc. Vapor Deposition Reactor For Forming Thin Film
US8470718B2 (en) 2008-08-13 2013-06-25 Synos Technology, Inc. Vapor deposition reactor for forming thin film
US8758512B2 (en) 2009-06-08 2014-06-24 Veeco Ald Inc. Vapor deposition reactor and method for forming thin film
US20110076421A1 (en) * 2009-09-30 2011-03-31 Synos Technology, Inc. Vapor deposition reactor for forming thin film on curved surface
US8840958B2 (en) 2011-02-14 2014-09-23 Veeco Ald Inc. Combined injection module for sequentially injecting source precursor and reactant precursor

Also Published As

Publication number Publication date
JPS6150892B2 (es) 1986-11-06
IT1120990B (it) 1986-03-26
DK305779A (da) 1980-01-21
JPS5515995A (en) 1980-02-04
NL7905581A (nl) 1980-01-22
DE2929092A1 (de) 1980-01-31
DK154823B (da) 1988-12-27
SE7906223L (sv) 1980-01-21
BE877465A (fr) 1980-01-04
DE2929092C2 (es) 1992-02-06
FR2456077B1 (es) 1983-04-22
FR2456077A1 (fr) 1980-12-05
NL189909B (nl) 1993-04-01
ES482995A1 (es) 1980-04-16
CA1138725A (en) 1983-01-04
NL189909C (nl) 1993-09-01
IT7968437A0 (it) 1979-07-11
SE440074B (sv) 1985-07-15
DK154823C (da) 1989-05-16

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